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Defluorination material and preparation and application thereof

A technology of fluorine materials and metal-organic frameworks, which is applied in the field of high-efficiency fluoride removal materials for zinc sulfate solution and its preparation, and can solve the problems of large amount of adsorbent, low selectivity of fluoride ions, and unsatisfactory fluoride removal effect of fluoride removal materials.

Inactive Publication Date: 2017-07-25
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The fluorine removal effect of the fluorine removal material disclosed in this patent document is not ideal
[0005] In summary, the commonly used adsorbents are used to remove fluoride from zinc sulfate solution, and there are disadvantages such as large interference, low selectivity to fluoride ions, and low fluoride removal efficiency, resulting in large amounts of adsorbents and difficulty in subsequent waste residue treatment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090] (1) Put 1.0g of UiO-66(Zr) in 100ml of methanol, after ultrasonic dispersion, let it stand for 20h, centrifuge, and vacuum dry at 120°C, then put it in a high-temperature oven at 200°C Keep it under 3h (activation).

[0091] (2) Dissolve 0.02g of magnesium nitrate, 0.01g of zirconium nitrate, 0.03g of aluminum nitrate, 0.02g of ferric nitrate, and 0.01g of lanthanum nitrate in 100ml of ethanol, place the activated material in step (1) in the solution, and ultrasonicate for 30min After that, fully stir for 12h. Then, ammonia solution was added while stirring to adjust the pH to 9, and stirring was continued for 1 h.

[0092] (3) The mixed sample in step (2) is centrifuged, washed 2-3 times, and vacuum-dried at 100° C. for 12 hours to obtain the fluorine-removing material of the present invention. The metal hydrate composition of the obtained fluorine removal material is Mg(OH) 2 0.81%; Zr(OH) 4 0.42%; Fe(OH) 3 0.84%; Al(OH) 3 1.24%; La(OH) 3 0.42%.

[0093] (...

Embodiment 2

[0095] (1) Dissolve 0.02g of magnesium nitrate, 0.01g of zirconium nitrate, 0.03g of aluminum nitrate, 0.02g of ferric nitrate, and 0.01g of lanthanum nitrate in 100ml of ethanol, put 1.0g of UiO-66(Zr) in the solution, and ultrasonically After 30min, fully stir for 12h. Then, ammonia solution was added while stirring to adjust the pH to 9, and stirring was continued for 1 h.

[0096] (2) The mixed sample in step (1) is centrifuged, washed 2-3 times, and vacuum-dried at 100° C. for 12 hours to obtain the fluorine-removing material of the present invention. The metal hydrate composition of the obtained fluorine removal material is Mg(OH) 2 0.21%; Zr(OH) 4 0.33%; Fe(OH) 3 0.25%; Al(OH) 3 0.45%; La(OH) 3 0.25%.

[0097](3) Use the prepared material to treat the zinc sulfate solution with a fluoride ion concentration of 125mg / L and a pH of 5.6 for 100min, and the dosage is 3g / L. After adsorption, the fluoride ion concentration drops to 52mg / L.

Embodiment 3

[0099] (1) Put 1.0g of UiO-66(Zr) in 100ml of methanol, after ultrasonic dispersion, let it stand for 20h, centrifuge, and vacuum dry at 120°C, then put it in a high-temperature oven at 200°C Keep it down for 3h.

[0100] (2) Dissolve 0.05g of magnesium nitrate and 0.04g of zirconium nitrate in 100ml of ethanol, place the material activated in step (1) in the solution, ultrasonicate for 30min, and then fully stir for 12h. Then, ammonia solution was added while stirring to adjust the pH to 9, and stirring was continued for 1 h. The composition of the obtained fluorine removal material is Mg(OH) 2 1.4%; Zr(OH) 4 0.95%.

[0101] (3) The mixed sample in step (2) is centrifuged, washed 2-3 times, and vacuum-dried at 100° C. for 12 hours to obtain the fluorine-removing material of the present invention. The metal hydrate composition of the obtained fluorine removal material is Mg(OH) 2 1.2%; Zr(OH) 4 0.92%.

[0102] (4) Treat the zinc sulfate solution with fluoride ion co...

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Abstract

The invention discloses a defluorination material, which comprises a metal organic framework material, wherein metal hydroxide is dispersed on the surface of the metal organic framework material and / or in holes; the metal hydroxide is at least one of Mg(OH)2, M(OH)3 and Zr(OH)4; and M is a trivalent metallic element. The invention further discloses the defluorination material which is obtained through activating the metal organic framework material at 180-260 DEG C, putting the metal organic framework material into a solution into which a water-soluble salt of magnesium, a water-soluble salt of M and a water-soluble salt of zirconium are dissolved, regulating the pH of a system to be 8.0-9.5 by using a fixing agent, carrying out stirring reaction, carrying out solid-liquid separation, washing and drying. In addition, the invention further discloses an application of the defluorination material in defluorination of a zinc sulfate solution. The preparation method of the defluorination material is simple, and the prepared material has large specific surface area and uniformly dispersed metal groups, has good compatibility on fluorin ions and has very high selectivity and high defluorination efficiency.

Description

technical field [0001] The invention belongs to the technical field of defluorination in the zinc smelting process, and in particular relates to a high-efficiency defluorination material for zinc sulfate solution in the hydrometallurgy industry and a preparation method thereof. Background technique [0002] Related reports show that more than 90% of metal zinc is produced by hydrometallurgy technology. However, in the production process, the excessive concentration of fluoride ions in the zinc sulfate solution will seriously affect the normal progress of the electrowinning process: the fluoride ions will destroy the oxide layer on the surface of the cathode aluminum plate and accelerate the consumption of the plate; The aluminum plate is bonded, which makes it difficult to strip zinc from the cathode, and also affects the quality of the electrolytic zinc. A series of hazards will increase the cost of the enterprise, reduce the production efficiency and affect the normal pro...

Claims

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Application Information

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IPC IPC(8): B01J20/22C02F1/28B01J20/30C02F101/14
CPCB01J20/041B01J20/06B01J20/226C02F1/288C02F2101/14
Inventor 田忠良郭伟昌张志剑杨超杨凯赖延清叶绍龙
Owner CENT SOUTH UNIV
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